CN105127666A - Method for ultrafine modification of surface of TC4 titanium alloy - Google Patents
Method for ultrafine modification of surface of TC4 titanium alloy Download PDFInfo
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- CN105127666A CN105127666A CN201510605164.1A CN201510605164A CN105127666A CN 105127666 A CN105127666 A CN 105127666A CN 201510605164 A CN201510605164 A CN 201510605164A CN 105127666 A CN105127666 A CN 105127666A
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Abstract
The invention provides a method for ultrafine modification of the surface of a TC4 titanium alloy. The method comprises the following steps: step S1 of selecting a flawless TC4 titanium alloy sample and performing polishing and straightening; step S2 of performing a groove in the surface of the TC4 titanium alloy so as to add silver particles; step S3 of fixing the TC4 titanium alloy with the added silver particles to a working table of a friction stir welding device, and performing machining under the protection of argon. Compared with the prior art, the method has the advantages that the method is executed on the surface of the TC4 titanium alloy, the shortcoming that the surface of the material is difficult to deform is overcome, crystal grains can be remarkably thinned by adding nanoscale silver particles, the biological activity of the surface of the material is improved, and the tissue infection after implantation is avoided.
Description
Technical field
What the present invention relates to is a kind of surface modifying method with the TC4 titanium alloy of nanometer enhancing silver particles for Srgery grafting field, agitating friction process for treating surface is specifically adopted to carry out strong plastic surface modification to Ti-6Al-4V, namely to the fine method of modifying of TC4 titanium alloy surface, by adding of nanometer-level silver particle, prepare nano combined biological medical titanium alloy.
Background technology
Phase early 1950s, at UK and USA, first pure titanium is used to manufacture the bio-medical materials such as bone plate, hip joint, intramedullary nail and screw.But clinical discovery, the intensity of the hip joint that pure titanium manufactures and intramedullary nail, rigidity is obviously not enough.After this, biomedical beta-titanium alloy material obtains huge development.At present, titanium alloy is the most noticeable bio-medical metallography material.; required by titanium alloy does not just have its mechanical property in the application of biomedical aspect, in addition, on the basis ensureing biological safety; also there is requirement more specifically to biocompatibility, corrosion resistance etc. with human body environment, and differ greatly in different aspect application.
Titanium alloy TC 4 material consist of Ti-6Al-4V, belong to alpha and beta type titan alloy, there is good comprehensive mechanics mechanical performance.Ti-6Al-4V alloy, due to many-sided excellent performance such as its high specific strength, low-density, biocompatibility, has been widely used in many industrial circles.But the surface abrasion of Ti-6Al-4V alloy is poor, in mechanical friction, have impact on the service life of product, and limit the application [3] of its such as hip implant etc. in bio-medical.The performance on its surface can be improved well to the Research on Surface Modification of Ti-6Al-4V alloy.In recent years, the develop rapidly at home of mixing yoghurt technology, it is a kind of novel material surface process technology, has broad application prospects.At home, the research of mixing yoghurt technology is mainly concentrated and the light-alloy such as magnalium, the intensity of the hardness of alloy surface, wearability and material monolithic can be improved and mould, toughness.And domestic mixing yoghurt technology is still in the starting stage in the research of bio-medical connection metal.Mixing yoghurt technology can carry out modification to TC4 titanium alloy surface, makes it have better mechanical property and surface property, and improves biocompatibility to a certain extent.But the infections relating of implant inevitably appears in postoperative syndrome, has bibliographical information, U.S.'s orthopaedics implant annual morbidity infected that is concerned with reaches 4.3%, becomes the main bugbear of puzzlement orthopaedics implant surgery.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of fine method of modifying to TC4 titanium alloy surface, the method is for prior art and application requirement, agitating friction process for treating surface (FSP) is applied in TC4 titanium alloy, realize material surface grain size, effective control of roughness, simultaneously by the anti-wear performance adding raising material surface and the biologically active of nanometer-level silver particle, avoid the bacteriological infection after implanting, Srgery grafting field can be widely used in.
The present invention is achieved by the following technical solutions:
The invention provides a kind of fine method of modifying to TC4 titanium alloy surface, it comprises the steps:
S1: choose flawless TC4 titanium alloy sample, carry out polishing and aligning;
S2: in described TC4 titanium alloy surface pre-groove to add Argent grain;
S3: filled out by Argent grain and be sprinkling upon in pre-groove, then on the workbench of agitating friction soldering equipment, under the protection of argon gas, processes.
Preferably, the smelting process of described TC4 titanium alloy is consumable electrode vacuum furnace melting.
Preferably, being operating as of described consumable electrode vacuum furnace melting:
After Ti-6Al-4V alloy being carried out three meltings, more than the beta transformation point of Ti-6Al-4V alloy, cogging forging is carried out to material, then carry out temperature Control Forging at the alpha+beta phase region of Ti-6Al-4V alloy, finally carry out hot rolling;
Wherein, described cogging forging temperature is 1010 ~ 1050 DEG C, and temperature Control Forging and hot-rolled temperature are 920 ~ 950 DEG C.
Preferably, the degree of depth of described groove is 0.5 ~ 2mm.
Preferably, described aligning employing four roller cold straightener.
Preferably, in step S3, the stirring-head process velocity of described agitating friction soldering equipment is 50mm/min, and Rotating speed is 225 ~ 375r/min.
Preferably, the average grain diameter of described Argent grain is 50nm.
Research shows, compared with other metal ions, and Ag
+there is very strong sterilizing ability, the infection after orthopaedics implantation can well be avoided.Therefore, nanoscale Ag particle is incorporated in the forced plasticity deforming of TC4 titanium alloy, makes material grains refinement, mechanical performance improve while, high degree avoid implant after an infection difficult problem.
Compared with prior art, the present invention has following beneficial effect:
Be carry out at TC4 titanium alloy surface by method of the present invention, overcome the shortcoming of this material surface difficulty distortion, adding after nanometer-level silver particle can remarkable crystal grain thinning, improves the biologically active of material surface, avoids the generation of implanting rear tissue infection.
Accompanying drawing explanation
By reading the detailed description done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the distribution (process velocity 50mm/min, Rotating speed 375r/min) of the TC4 surface A g particle layer after 1 passage stirs;
Fig. 2 is product and the control sample nano impress loading curve figure of embodiment 1;
Fig. 3 is the SEM figure of corresponding impression in Fig. 2;
Fig. 4 is the result of the test figure after staphylococcus aureus is seeded in product and control sample respectively;
Fig. 5 is the antibiotic rate figure adding silver-colored sample.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
Adopt agitating friction surface treatment to the modification of TC4 titanium alloy surface, concrete steps are as follows:
A prepared by (), material: adopt intermediate alloy additive by composition proportion weighing, utilize vacuum consumable smelting technology three melting Ti-6Al-4V (wt%) titanium alloys repeatedly, melt out the ingot casting of diameter 80 ~ 120mm.Forge material 1050 DEG C and 950 DEG C respectively, be forged into the square billet of thickness at 30 ~ 50mm, carry out hot rolling after abrasive material blemish at 950 DEG C to material, pass deformation controls 5 ~ 8%, is rolled down to thickness about 4 ~ 6mm;
The flaw detection of (b), material, surface treatment: be the TC4 titanium alloy surface polishing scale removal of about 4 ~ 6mm by thickness after rolling, adopt four roller cold straighteners to align material, adopt the defects such as ultrasonic examination determination material pore-free, with sander, material surface is polished down to smooth state;
(c), design surface groove: be that the groove of 0.5mm is to add Argent grain in the prefabricated degree of depth of TC4 titanium alloy surface;
(d), installation processing sample: sample fixture is fixed on the workbench of agitating friction soldering equipment, and sets each technological parameter of processing; The technological parameter of design mixing yoghurt: process velocity 50 ~ 100mm/min, Rotating speed 225 ~ 375r/min, controlling the shaft shoulder press-in surface of the work degree of depth in process is 0.3 ~ 0.5mm;
(e), material surface process: to confirming in step (d) that flawless TC4 titanium alloy carries out surface stirring friction surface modification; Processing technology, as shown in step (d), with argon shield in process, processes 1 passage.
The impression performance of the TC4 titanium alloy after the present embodiment surface modification is as shown in table 1:
The performance data of table 1 impression
Point 1 is positioned at argentiferous position, and puts the position that 2 are positioned at not argentiferous.The specific performance of 2 is illustrated in table.Obviously, the hardness of point 1 improves 30.71% nearly compared to point 2, and reach 5.31GPa, ultimate depth is also shallow than point 2.From SEM figure, obviously can see, put in 1 impression and in neighbouring matrix and be uniform-distribution with nano-Ag particles, and put the distribution not seeing Argent grain in 2.This illustrates, nano-Ag particles evenly adds in matrix, effectively can improve matrix hardness.But also can see from table, elastic modelling quantity has almost no change, and point 1 only improves 1.37% than point 2.This illustrates the interpolation of soft nano-Ag particles, although dislocation motion this respect can be hindered to improve the hardness of matrix from distortion of lattice, do not significantly improve the elastic modelling quantity of matrix, this has certain effect for the stress shielding effect reducing metal implant.
As shown in Figure 2, the stereoscan photograph of corresponding impression as shown in Figure 3 for the nano impress loading curve figure of the product that the present embodiment obtains and control sample.
S. aureus Inoculate in two kinds of long time without surface modification and the live/dead coloration result after material surface 6h and 24h of surface modification is: the biomembrane that viable bacteria is formed presents green, dead bacterium and impaired biomembrane present as can see from Figure 4 red, along with incubation time extends to 24h from 6h, the green fluorescence intensity (bacterial multiplication of living) on TC4 surface is in increase, and the green fluorescence intensity on Ag-TC4 surface declines, red fluorescence increases on the contrary.This shows, after nano-Ag particles introduces TC4 surface, it has good antibacterial activity.
Antibiotic rate (Ra) is used for evaluating number of viable on Ag-TC4 surface after Bacteria Culture inoculation 6h and 24h
Ra(％)＝(A-B)/A*100％
The mean viable quantity of A representative on TC4 surface, the mean viable quantity of B representative on Ag-TC4 surface.As can be seen from Figure 5 no matter be reach more than 90% at the antibiotic rate on 6h or 24h, Ag-TC4 surface, surface Ag-TC4 can the adhesion of anti-bacteria and propagation.
embodiment 2
Adopt agitating friction surface treatment to the modification of TC4 titanium alloy surface, concrete steps are as follows:
The prefabricated degree of depth of TC4 titanium alloy surface be the groove of 1mm to add Argent grain, other conditions, with embodiment 1, carry out 1 passage distortion in argon atmosphere.
embodiment 3
Adopt agitating friction surface treatment to the modification of TC4 titanium alloy surface, concrete steps are as follows:
The prefabricated degree of depth of TC4 titanium alloy surface be the groove of 1.5mm to add Argent grain, other conditions, with embodiment 1, carry out 1 passage distortion in argon atmosphere; Figure 1 shows that process velocity 50mm/min, the distribution of the TC4 surface A g particle layer after Rotating speed 375r/min1 passage stirs.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (8)
1., to a fine method of modifying for TC4 titanium alloy surface, it is characterized in that, comprise the steps:
S1: choose flawless TC4 titanium alloy sample, carry out polishing and aligning;
S2: in described TC4 titanium alloy surface pre-groove to add Argent grain;
S3: filled out by Argent grain and be sprinkling upon in pre-groove, then on the workbench of agitating friction soldering equipment, under the protection of argon gas, processes.
2. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, it is characterized in that, the smelting process of described TC4 titanium alloy is consumable electrode vacuum furnace melting.
3. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 2, is characterized in that, being operating as of described consumable electrode vacuum furnace melting:
After Ti-6Al-4V alloy being carried out three meltings, more than the beta transformation point of Ti-6Al-4V alloy, cogging forging is carried out to material, then carry out temperature Control Forging at the alpha+beta phase region of Ti-6Al-4V alloy, finally carry out hot rolling;
Wherein, described cogging forging temperature is 1010 ~ 1050 DEG C, and temperature Control Forging and hot-rolled temperature are 920 ~ 950 DEG C.
4. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, it is characterized in that, the degree of depth of described groove is 0.5 ~ 2mm.
5. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, is characterized in that, described aligning employing four roller cold straightener.
6. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, it is characterized in that, in step S3, the stirring-head process velocity of described agitating friction soldering equipment is 50mm/min, and Rotating speed is 225 ~ 375r/min.
7. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, it is characterized in that, in step S3, the shaft shoulder pressing in sample case depth controlling described agitating friction soldering equipment is 0.3 ~ 0.5mm.
8. the fine method of modifying to TC4 titanium alloy surface as claimed in claim 1, it is characterized in that, the average grain diameter of described Argent grain is 50nm.
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Cited By (3)
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| CN107442878A (en) * | 2017-07-31 | 2017-12-08 | 南昌大学 | A kind of TC4 titanium alloy surface method of modifying based on soldering in situ |
| CN108754371A (en) * | 2018-05-24 | 2018-11-06 | 太原理工大学 | A kind of preparation method refining nearly α high-temperature titanium alloys crystal grain |
| CN108823368A (en) * | 2018-07-05 | 2018-11-16 | 燕山大学 | A kind of hot-working method of carbon evanohm |
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Cited By (4)
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|---|---|---|---|---|
| CN107442878A (en) * | 2017-07-31 | 2017-12-08 | 南昌大学 | A kind of TC4 titanium alloy surface method of modifying based on soldering in situ |
| CN107442878B (en) * | 2017-07-31 | 2019-12-20 | 南昌大学 | TC4 titanium alloy surface modification method based on in-situ brazing |
| CN108754371A (en) * | 2018-05-24 | 2018-11-06 | 太原理工大学 | A kind of preparation method refining nearly α high-temperature titanium alloys crystal grain |
| CN108823368A (en) * | 2018-07-05 | 2018-11-16 | 燕山大学 | A kind of hot-working method of carbon evanohm |
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Application publication date: 20151209 |